Method for extracting tungsten from alkaline crude sodium tungstate solution without renewable recyclable extracting system

A crude sodium tungstate and extraction technology, which is applied in the field of tungsten hydrometallurgy, can solve the problems that the regeneration liquid cannot be directly returned to the main process, consume large alkali, and the cost of the process is short, and achieves the effect of eliminating the regeneration process.

Active Publication Date: 2015-05-20
CENT SOUTH UNIV
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  • Abstract
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  • Claims
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Problems solved by technology

[0015] The present invention aims at the disadvantages of the quaternary ammonium carbonate alkaline extraction method of tungsten in the prior art that a large amount of alkali needs to be consumed in the regeneration process, and the regeneration liquid cannot be directly returned to the main process, and the purpose is to provide a short process flow and low cost A method of directly and selectively extracting tungstate ions from alkaline crude sodium tungstate solution to produce pure ammonium tungstate by a recyclable extraction system without regeneration; this method realizes that the extractant can be directly reused without regeneration, reducing the Chemical reagent consumption, environmental protection and reduced production costs, conducive to industrial production

Method used

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  • Method for extracting tungsten from alkaline crude sodium tungstate solution without renewable recyclable extracting system
  • Method for extracting tungsten from alkaline crude sodium tungstate solution without renewable recyclable extracting system
  • Method for extracting tungsten from alkaline crude sodium tungstate solution without renewable recyclable extracting system

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Feed liquid: The feed liquid is low-grade scheelite soda high-pressure leaching liquid, of which WO 3 10.0g / L, P0.10g / L, As0.02g / L, Si0.1g / L, Na 2 CO 3 21.5g / L.

[0036] Organic phase: The organic phase is 60% methyl trioctyl ammonium chloride + 25% 2-octanol + 15% sulfonated kerosene (volume percentage). Before extraction, pre-mix the organic phase with 2.5mol / L NH 4 HCO 3 -1.0mol / L(NH 4 ) 2 CO 3 Mixed ammonium solution is carried out multi-stage cross-flow treatment by comparing 2 / 1, makes the methyl trioctyl ammonium chloride in the organic phase completely convert to the bicarbonate of methyl trioctyl ammonium and the mixture of carbonate, wherein The molar ratio of bicarbonate to carbonate is about 8:1.

[0037] Operation: The above-mentioned organic phase and feed liquid are subjected to 8-stage countercurrent extraction at a flow ratio of 1 / 10, and the negative tungsten organic phase is subjected to 3-stage countercurrent washing with deionized water at a...

Embodiment 2

[0040] Feed liquid: Feed liquid is wolframite sodium hydroxide leaching liquid, in which WO3300.0g / L, P1.50g / L, As0.70g / L, Si0.75g / L, NaOH70g / L.

[0041] Organic phase: The organic phase is 25% N263 + 20% 2-octanol + 55% aviation kerosene (volume percentage). N263 is the product code of domestic quaternary ammonium salt extractant, which is a kind of methyl trialkylammonium chloride, in which the carbon atoms in the three alkyl groups are 8-10 respectively. The organic phase was mixed with 1.0mol / L NH several times before extraction 4 HCO 3 -0.5mol / L(NH 4 ) 2 CO 3 The mixed ammonium solution is contacted to convert the methyltrialkylammonium chloride in the organic phase to a mixture of bicarbonate and carbonate of methyltrialkylammonium, wherein the molar ratio of bicarbonate to carbonate is about 6 :1.

[0042] Operation: The above organic phase and feed liquid are subjected to 15-stage countercurrent extraction under the condition of a flow ratio of 10 / 1, and the nega...

Embodiment 3

[0045] Feed liquid: The feed liquid is scheelite soda high pressure leaching liquid, in which WO 3 130.3g / L, P0.020g / L, As0.012g / L, Si0.035g / L, Na 2 CO 3 100.2g / L.

[0046] Organic phase: The organic phase is 10% methyl trinonyl ammonium chloride + 20% sec-octanol + 70% No. 260 solvent oil (volume percentage). Before the extraction, the organic phase was mixed with 2.2mol / L NH 4 HCO 3 -1.2mol / L(NH 4 ) 2 CO 3 The mixed ammonium solution is contacted to convert the methyltrinonylammonium chloride in the organic phase into a mixture of bicarbonate and carbonate of methyltrinonylammonium, wherein the molar ratio of bicarbonate to carbonate is about 5.5 :1.

[0047] Operation: The above-mentioned organic phase and the feed liquid are subjected to 9-stage countercurrent extraction at a flow ratio of 8 / 1, and the negative tungsten organic phase is subjected to 5-stage countercurrent washing with deionized water at a flow ratio of 6 / 1, and then washed with 2.2mol / L NH 4 HCO ...

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Abstract

The invention discloses a method for extracting tungsten from alkaline crude sodium tungstate solution without regenerating a recyclable extraction system; the method uses bicarbonate containing methyltrialkylammonium and its carbonate composite extractant The organic phase is subjected to multi-stage countercurrent extraction with respect to the alkaline crude sodium tungstate solution, and the obtained loaded organic phase is washed with water and then subjected to multi-stage counter-current back extraction with a mixed aqueous solution of ammonium bicarbonate and ammonium carbonate to obtain ammonium tungstate solution. The phase is directly returned to the extraction process for repeated use; this method can selectively extract tungstate ions from alkaline crude sodium tungstate solution to prepare ammonium tungstate, which realizes the effective separation of tungstate ions and impurity ions containing phosphorus, arsenic, silicon, etc. Separation, and more importantly, the extraction agent can be directly reused without regeneration, which shortens the process flow, reduces the consumption of chemical reagents, and reduces waste water discharge, which is beneficial to industrial production.

Description

technical field [0001] The invention relates to a method for extracting tungsten from an alkaline crude sodium tungstate solution without regeneration and a recyclable extraction system, which belongs to the field of tungsten hydrometallurgy. Background technique [0002] Tungsten is a rare metal element with a wide range of uses. Industrially, tungsten is extracted from various tungsten-containing materials, including tungsten mineral resources (such as scheelite, wolframite and black and white tungsten mixed ore, etc.), secondary resources of tungsten (such as waste tungsten-containing catalysts, etc.) And various intermediate materials in the process of tungsten industry (such as crude tungstic acid), etc. [0003] Sodium hydroxide leaching method or soda high-pressure leaching method is widely used in industry to leach tungsten from tungsten-containing materials to obtain alkaline crude sodium tungstate solution. The crude sodium tungstate solution contains not only so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B34/36C22B3/28
CPCY02P10/20
Inventor 张贵清肖连生关文娟张启修李青刚陈世梁
Owner CENT SOUTH UNIV
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